CN103305702B - Process for recovering and purifying neptunium from waste liquor discharged from 2AW+2DW in Purex flow - Google Patents
Process for recovering and purifying neptunium from waste liquor discharged from 2AW+2DW in Purex flow Download PDFInfo
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Abstract
The invention belongs to the technical field of nuclear fuel reprocessing and discloses a process for recovering and purifying neptunium from waste liquor discharged from 2AW+2DW in Purex flow. The process comprises the primary neptunium purification process and the secondary neptunium purification process; the process comprises the following steps: by taking 30 volume percent of TBP-kerosene as an extraction agent, extracting Np, U and Pu to the organic phase, and allowing the fission fragments to enter the aqueous phase; adding a reducing agent and an extraction agent into the organic phase, reversely extracting the Np to the aqueous phase; further extracting uranium and plutonium, and performing oxalate precipitation, filtering and calcining on the obtained aqueous phase product to obtain the purified neptunium oxide solid. The process has the advantages that the neptunium recovery rate is over 98 percent, and the uranium and plutonium removal coefficient in neptunium is high.
Description
Technical field
The invention belongs to nuclear fuel reprocessing technical field, be specifically related to a kind of technique of recovery and purifying neptunium from the 2AW+2DW intermediate level liquid waste of Purex flow.
Background technology
In spent fuel, neptunium content is about 500 ~ 700 grams/ton, wherein
237the irradiation products of Np is
238pu is important αsource, has purposes widely.Current reprocessing plant extracts neptunium substantially to be had and to extract from high activity liquid waste and intermediate level liquid waste extracts two kinds of approach, and the technique of extraction neptunium mainly contains ion exchange method and solvent extration.The principle of its ion exchange methods is under high density nitric acid condition, utilizes neptunium, plutonium, avidity between fission product from ion exchange resin different, realizes neptunium, plutonium is separated with fission product; Then use and carry out reductive desorption plutonium as reagent such as ferrous irons, finally adopt low acidolysis suction neptunium, finally realize being separated of plutonium and neptunium.In order to purifying neptunium, also may need the cyclical operation carrying out second time or third time, the shortcoming of employing ion exchange method is complex operation and the nuclear waste such as the waste liquid produced and spent resin is many.The Jiang Hao of Institute for Atomic Research etc. disclose " from Purex flow intermediate level liquid waste reclaim and purifying neptunium, plutonium, uranium research ", disclose in literary composition and utilize solvent extration to reclaim the neptunium in 2AW and 2DW, plutonium, uranium, TBP is as extraction agent, with hydrogen peroxide, hydrazine nitrate-Sodium Nitrite, hydrazine nitrate-hydroxylamine nitriate-nitrosonitric acid make redox agent, quantified extract neptunium, plutonium, uranium.But due to the more subsequent disposal being unfavorable for feed liquid of kind of redox agent used, and it is selected in reductive agent and has Sodium Nitrite, this be also do not wish in aftertreatment to use have salt reductive agent, be therefore not suitable for for purifying and neptunium recovery.
Summary of the invention
(1) goal of the invention
Problem existing for prior art, the invention provides that a kind of neptunium rate of recovery removes uranium up to more than 98%, in neptunium, the neptunium that goes plutonium coefficient high reclaims and purifying process.
(2) technical scheme
In order to solve the problem existing for prior art, technical scheme provided by the invention is as follows:
Reclaim and the technique of purifying neptunium from the 2AW+2DW intermediate level liquid waste of Purex flow, this technique comprises the first time purifying process and the second time purifying process of neptunium of neptunium, and wherein the first time purifying process of neptunium comprises the following steps:
(1) by after plutonium extraction tank raffinate 2AW and uranium extraction groove raffinate 2DW evaporation concentration, with sodium metavanadate as oxygenant condiment, 5 ~ 10mol/L HNO
3regulate acidity, obtain feed liquid 2NAF to be purified, wherein comprise Np, U, Pu and fission product in 2NAF, Np is mainly with Np(VI) form existence;
(2) 2NAF is introduced in neptunium extraction tank 2NA, also introduce 30%TBP-kerosene (volume fraction) in 2NA as extraction agent 2NAX, 3 ~ 4mol/L HNO
3as washing composition 2NAS, wherein U, Np, Pu jointly extract and enter organic phase 2NAP, and fission product enters aqueous phase 2NAW;
(3) the organic phase 2NAP obtained in step (2) is incorporated in neptunium back extraction groove 2NB as 2NBF, in 2NB groove, also introduces 0.2 ~ 0.5mol/L hydrazine or hydrazine derivative-0.2 ~ 0.4 mol/L HNO
3as reduction reextraction agent 2NBX, hydrazine wherein in reduction reextraction agent or hydrazine derivative are by Np(VI) be reduced to Np(V), Np is from organic phase back extraction to aqueous phase, and 30%TBP-kerosene (volume fraction) is as mending the further Extraction of Uranium of extraction agent 2NBS, plutonium, and water-phase product is 2NBP;
The second time purifying process of neptunium comprises the following steps:
(1) in 2NBP feed liquid, add liquid nitrogen tetroxide, destroy hydrazine reducing agent wherein or hydrazine derivative, as oxygenant, Np is oxidized to sexavalence with sodium metavanadate, with 5 ~ 10mol/L HNO
3regulate concentration of nitric acid in 2NBP to be 4mol/L, then 2NBP is entered into the extraction tank 3NA of the second time purifying process of neptunium as 3NAF feed liquid;
(2) 3NAF is introduced in neptunium extraction tank 3NA, also introduce 30%TBP-kerosene (volume fraction) in 3NA as extraction agent 3NAX, 3 ~ 4mol/L HNO
3as washing composition 3NAS, wherein U, Np, Pu jointly extract and enter organic phase 3NAP, and fission product enters aqueous phase 3NAW;
(3) the organic phase 3NAP obtained in step (2) is incorporated in neptunium back extraction groove 3NB as 3NBF, in 3NB groove, also introduces 0.2 ~ 0.5mol/L hydrazine or hydrazine derivative-0.2 ~ 0.4 mol/LHNO
3as reduction reextraction agent 3NBX, hydrazine wherein in reduction reextraction agent or hydrazine derivative are by Np(VI) be reduced to Np(V), Np is from organic phase back extraction to aqueous phase, and 30%TBP-kerosene (volume fraction) is as mending the further Extraction of Uranium of extraction agent 3NBS, plutonium, and water-phase product is 3NBP;
(4) by 3NBP 4 ~ 6mol/L HNO
3, after 0.5 ~ 0.7mol/L hydrazine or hydrazine derivative condiment, add the oxalic acid of 0.5 ~ 1.2 mol/L and make oxalic acid surplus 0.05 ~ 0.15mol/L, under 50 ~ 60 DEG C of conditions, obtaining neptunium oxalate precipitation, and after filtration, obtain neptunium dioxide solid after calcining;
(5) mother liquor after filtration in step (4) is mixed with 2NBP after evaporation concentration, then operate according to step (1), (2) (3), (4) successively.
Preferably, the stream of the stream ratio of 2NAX:2NAF:2NAS, 2NBS:2NBF:2NBX is 1:3:1 than for, the stream ratio of 3NAX:3NAF:3NAS and the stream ratio of 3NBS:3NBF:3NBX.
Preferably, in the step (4) of second time purifying process, described calcining is divided into three phases: the first stage: temperature from ambient rises to 100 DEG C, removes the free water in neptunium oxalate precipitation; Subordinate phase: temperature, at 100 DEG C ~ 200 DEG C, removes the crystal water in neptunium oxalate precipitation; Phase III: 300 ~ 320 DEG C, neptunium oxalate resolves into neptunium dioxide.
Preferably, the step (3) of purifying process, the middle reduction reextraction agent of step (3) of second time purifying process are 0.2 ~ 0.5mol/L hydrazine-0.2 ~ 0.4 mol/LHNO for the first time
3, with 4 ~ 6mol/L HNO in the step (4) of second time purifying process
3, 0.5 ~ 0.7mol/L hydrazine condiment.
(3) beneficial effect
The technique of recovery provided by the invention and purifying neptunium, the rate of recovery of neptunium is up to more than 98%, and it also has the following advantages: (1), in twice purifying process, all devises and mends extraction step, namely devise 30%TBP-kerosene respectively as the agent of benefit extraction at 2NB, 3NB groove, uranium, plutonium can be extracted further.
(2) at needs by Np by Np(V) be oxidizing to Np(VI) in process, all add sodium metavanadate as stablizer and oxygenant, be conducive to the raising of the neptunium rate of recovery.
For the step of first time purifying process (1), because in 2AW and 2DW, neptunium is mainly tetravalence and pentavalent two kinds of valence states, but neptunium only has hexavalent form effectively could be extracted by TBP, in technique in the past, require that the neptunium of more than 99% can be oxidized to sexavalence, this is very difficult and is be difficult to realize in actually operating, and in this technique, only need the neptunium of more than 90% to be oxidized to sexavalence, equally also can realize the yield of more than 98%.Reason adds sodium metavanadate, concrete principle is: pentavalent neptunium can be oxidizing to sexavalence and can make Np(VI by adding of sodium metavanadate) valence stability, at 30%TBP-kerosene (volume fraction) constantly extraction Np(VI) process in the middle of, due to chemical equilibrium relation, Np(V) also can constantly by VO
3 -be oxidized to Np(VI), then constantly extracted by TBP, so the neptunium of more than 99.9% is all extracted in 2NA groove.In the step (1) of second time purifying process, also add sodium metavanadate, its mechanism of action is similar to above-mentioned.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of recovery and purifying Np from 2AW+2DW;
Fig. 2 is the first time purifying process figure of Np;
Fig. 3 is the second time purifying process figure of Np.
Embodiment
Below in conjunction with specification drawings and specific embodiments, the present invention is further elaborated.
embodiment 1
Be installed on by experimental stand in glove box, reclaim and purifying the neptunium in plutonium extraction tank raffinate 2AW and uranium extraction groove raffinate 2DW feed liquid, its operation steps is:
(1) by after plutonium extraction tank raffinate 2AW and uranium extraction groove raffinate 2DW evaporation concentration, with sodium metavanadate as oxygenant condiment, the HNO of 5mol/L
3regulate acidity, obtain feed liquid 2NAF to be purified, wherein comprise Np, U, Pu and fission product in 2NAF, Np is mainly with Np(VI) form existence;
(2) 2NAF is introduced in neptunium extraction tank 2NA, also introduce 30%TBP-kerosene (volume fraction) in 2NA as extraction agent 2NAX, 3mol/L HNO
3as washing composition 2NAS, wherein U, Np, Pu jointly extract and enter organic phase 2NAP, and fission product enters aqueous phase 2NAW, and the stream of 2NAX:2NAF:2NAS is than being 1:3:1.
(3) the organic phase 2NAP obtained in step (2) is incorporated in neptunium back extraction groove 2NB as 2NBF, in 2NB groove, also introduces 0.2mol/L hydrazine-0.2 mol/LHNO
3as reduction reextraction agent 2NBX, hydrazine wherein in reduction reextraction agent is by Np(VI) be reduced to Np(V), Np is from organic phase back extraction to aqueous phase, 30%TBP-kerosene (volume fraction) is as mending the further Extraction of Uranium of extraction agent 2NBS, plutonium, water-phase product is that the stream of 2NBP, 2NBS:2NBF:2NBX is than being 1:3:1;
The second time purifying process of neptunium comprises the following steps:
(1) in 2NBP feed liquid, add liquid nitrogen tetroxide, destroy hydrazine reducing agent wherein, as oxygenant, Np is oxidized to sexavalence with sodium metavanadate, uses 5mol/L HNO
3regulate concentration of nitric acid in 2NBP to be 4mol/L, then 2NBP is entered into the extraction tank 3NA of the second time purifying process of neptunium as 3NAF feed liquid;
(2) 3NAF is introduced in neptunium extraction tank 3NA, also introduce 30%TBP-kerosene (volume fraction) in 3NA as extraction agent 3NAX, 3mol/L HNO
3as washing composition 3NAS, wherein U, Np, Pu jointly extract and enter organic phase 3NAP, and fission product enters aqueous phase 3NAW, and the stream of 3NAX:3NAF:3NAS is than being 1:3:1;
(3) the organic phase 3NAP obtained in step (2) is incorporated in neptunium back extraction groove 3NB as 3NBF, in 3NB groove, also introduces 0.2mol/L hydrazine-0.2 mol/LHNO
3as reduction reextraction agent 3NBX, hydrazine wherein in reduction reextraction agent is by Np(VI) be reduced to Np(V), Np is from organic phase back extraction to aqueous phase, 30%TBP-kerosene (volume fraction) is as mending the further Extraction of Uranium of extraction agent 3NBS, plutonium, water-phase product is that the stream ratio of 3NBP, 3NBS:3NBF:3NBX is 1:3:1;
(4) 3NBP is used 4mol/L HNO
3, after 0.5mol/L hydrazine condiment, add the oxalic acid of 0.5 mol/L and make the superfluous 0.05mol/L of oxalic acid, under 50 DEG C of conditions, obtaining neptunium oxalate precipitation, and after filtration, obtain neptunium dioxide solid after calcining; Described calcining is divided into three phases: the first stage: temperature from ambient rises to 100 DEG C, removes the free water in neptunium oxalate precipitation; Subordinate phase: temperature, at 100 DEG C ~ 200 DEG C, removes the crystal water in neptunium oxalate precipitation; Phase III: 300 ~ 320 DEG C, neptunium oxalate resolves into neptunium dioxide.
(5) mother liquor after filtration in step (4) is mixed with 2NBP after evaporation concentration, then operate according to step (1), (2) (3), (4) successively.
Rig test result is: the rate of recovery of neptunium is 99.92%.
embodiment 2
Identical with method with the operation steps in embodiment 1, unlike Parameters variation such as condiment concentration, reductant concentrations, table specific as follows:
Table 1 parameter list
embodiment 3
Identical with method with the operation steps in embodiment 1, unlike the condiment parameter in the step (4) of second time purifying process and concentration of oxalic acid, be specially 3NBP 5mol/L HNO
3, 0.6 mol/L hydrazine condiment, add 1.0mol/L oxalic acid and make the superfluous 0.1mol/L of oxalic acid, carry out oxalate precipitation, the rate of recovery of neptunium is 99.91%.
embodiment 4
Identical with method with the operation steps in embodiment 1, unlike the condiment parameter in the step (4) of second time purifying process and concentration of oxalic acid, be specially 3NBP 6mol/L HNO
3, 0.7 mol/L hydrazine condiment, add 1.2mol/L oxalic acid and make the superfluous 0.15mol/L of oxalic acid, carry out oxalate precipitation, the rate of recovery of neptunium is 99.91%.
embodiment 5
Identical with step with embodiment 1 method therefor, unlike the hydrazine replaced with hydrazine derivative in embodiment 1, rig test result is: the rate of recovery of neptunium is 99.83%.
Claims (3)
1. reclaim and the technique of purifying neptunium from the 2AW+2DW intermediate level liquid waste of Purex flow, it is characterized in that, this technique comprises the first time purifying process and the second time purifying process of neptunium of neptunium, and wherein the first time purifying process of neptunium comprises the following steps:
(1) by after plutonium extraction tank raffinate 2AW and uranium extraction groove raffinate 2DW evaporation concentration, with sodium metavanadate as oxygenant condiment, 5 ~ 10mol/L HNO
3regulate acidity, obtain feed liquid 2NAF to be purified, wherein comprise Np, U, Pu and fission product in 2NAF, Np mainly exists with Np (VI) form;
(2) 2NAF is introduced in neptunium extraction tank 2NA, also introduce in 2NA 30%TBP ?kerosene (volume fraction) as extraction agent 2NAX, 3 ~ 4mol/L HNO
3as washing composition 2NAS, wherein U, Np, Pu jointly extract and enter organic phase 2NAP, and fission product enters aqueous phase 2NAW;
(3) the organic phase 2NAP obtained in step (2) is incorporated in neptunium back extraction groove 2NB as 2NBF, in 2NB groove, also introduces 0.2 ~ 0.5mol/L hydrazine or hydrazine derivative-0.2 ~ 0.4mol/L HNO
3as reduction reextraction agent 2NBX, Np (VI) is reduced to Np (V) by the hydrazine wherein in reduction reextraction agent or hydrazine derivative, Np is from organic phase back extraction to aqueous phase, 30%TBP ?kerosene (volume fraction) as mending extraction agent 2NBS further Extraction of Uranium, plutonium, water-phase product is 2NBP;
The second time purifying process of neptunium comprises the following steps:
(1) in 2NBP feed liquid, add liquid nitrogen tetroxide, destroy hydrazine reducing agent wherein or hydrazine derivative, as oxygenant, Np is oxidized to sexavalence with sodium metavanadate, with 5 ~ 10mol/L HNO
3regulate concentration of nitric acid in 2NBP to be 4mol/L, then 2NBP is entered into the extraction tank 3NA of the second time purifying process of neptunium as 3NAF feed liquid;
(2) 3NAF is introduced in neptunium extraction tank 3NA, also introduce in 3NA 30%TBP ?kerosene (volume fraction) as extraction agent 3NAX, 3 ~ 4mol/L HNO
3as washing composition 3NAS, wherein U, Np, Pu jointly extract and enter organic phase 3NAP, and fission product enters aqueous phase 3NAW;
(3) the organic phase 3NAP obtained in step (2) is incorporated in neptunium back extraction groove 3NB as 3NBF, in 3NB groove, also introduces 0.2 ~ 0.5mol/L hydrazine or hydrazine derivative-0.2 ~ 0.4mol/L HNO
3as reduction reextraction agent 3NBX, Np (VI) is reduced to Np (V) by the hydrazine wherein in reduction reextraction agent or hydrazine derivative, Np is from organic phase back extraction to aqueous phase, 30%TBP ?kerosene (volume fraction) as mending extraction agent 3NBS further Extraction of Uranium, plutonium, water-phase product is 3NBP;
(4) by 3NBP 4 ~ 6mol/L HNO
3, after 0.5 ~ 0.7mol/L hydrazine or hydrazine derivative condiment, add the oxalic acid of 0.5 ~ 1.2mol/L and make oxalic acid surplus 0.05 ~ 0.15mol/L, under 50 ~ 60 DEG C of conditions, obtaining neptunium oxalate precipitation, and after filtration, obtain neptunium dioxide solid after calcining;
(5) mother liquor after filtration in step (4) is mixed with 2NBP after evaporation concentration, then operate according to step (1), (2) (3), (4) successively;
In above-mentioned technique, the stream ratio of 2NAX:2NAF:2NAS, the stream ratio of 2NBS:2NBF:2NBX, the stream ratio of 3NAX:3NAF:3NAS and the stream ratio of 3NBS:3NBF:3NBX are 1:3:1.
2. the technique of a kind of recovery and purifying neptunium from the 2AW+2DW intermediate level liquid waste of Purex flow according to claim 1, it is characterized in that, in the step (4) of second time purifying process, described calcining is divided into three phases: the first stage: temperature from ambient rises to 100 DEG C, removes the free water in neptunium oxalate precipitation; Subordinate phase: temperature, at 100 DEG C ~ 200 DEG C, removes the crystal water in neptunium oxalate precipitation; Phase III: 300 ~ 320 DEG C, neptunium oxalate resolves into neptunium dioxide.
3. the technique of a kind of recovery and purifying neptunium from the 2AW+2DW intermediate level liquid waste of Purex flow according to claim 1, it is characterized in that, the step (3) of purifying process, the middle reduction reextraction agent of step (3) of second time purifying process are 0.2 ~ 0.5mol/L hydrazine-0.2 ~ 0.4mol/L HNO for the first time
3, with 4 ~ 6mol/L HNO in the step (4) of second time purifying process
3, 0.5 ~ 0.7mol/L hydrazine condiment.
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| CN105110487B (en) * | 2015-09-06 | 2017-10-31 | 中国人民解放军63653部队 | The microorganism of plutonium removes and recovery method in a kind of acid waste water |
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| RU2691132C1 (en) * | 2018-07-26 | 2019-06-11 | Акционерное общество "Высокотехнологический научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара" | Method of plutonium extraction and purification |
| CN112071461B (en) * | 2020-09-03 | 2022-11-18 | 清华大学 | Treatment method of high-fuel-consumption high-radioactivity waste liquid |
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